Use of a composition

ABSTRACT

There is provided use of a pectin composition to prepare an aqueous composition having high yield stress characteristics without substantial gelation, wherein the pectin composition comprises at least a population of pectin that is calcium sensitive; wherein the pectin composition is capable of imparting high yield stress characteristics to an aqueous composition without causing substantial gelation of the aqueous composition.

[0001] The present invention relates to a use of a composition. Inparticular, the present invention relates to a use of a pectincomposition.

[0002] Pectin is an important commodity in today's industry. Forexample, it can be used in the food industry as a thickening or gellingagent, such as in the preparation of jams or fruit systems for yoghurt.

[0003] Pectin is a structural polysaccharide commonly found in the formof protopectin in plant cell walls. The backbone of pectin comprisesα-1-4 linked galacturonic acid residues which are interrupted with asmall number of 1,2 linked α-L-rhamnose units. In addition, pectincomprises highly branched regions with an almost alternatingrhamno-galacturonan chain. These highly branched regions also containother sugar units (such as D-galactose, L-arabinose and xylose) attachedby glycosidic linkages to the C3 or C4 atoms of the rhamnose units orthe C2 or C3 atoms of the galacturonic acid units. The long chains ofα-1-4 linked galacturonic acid residues are commonly referred to as“smooth” regions, whereas the highly branched regions are commonlyreferred to as the “hairy regions”.

[0004] Some of the carboxyl groups of the galacturonic residues areesterified (e.g. the carboxyl groups are methylated). Typicallyesterification of the carboxyl groups occurs after polymerisation of thegalacturonic acid residues. However, it is extremely rare for all of thecarboxyl groups to be esterified (e.g. methylated). Usually, the degreeof esterification will vary from 0-90%. If more than 50% of the carboxylgroups are esterified then the resultant pectin is referred to as a“high ester pectin” (“HE pectin” for short) or a “high methoxyl pectin”.If less than 50% of the carboxyl groups are esterified then theresultant pectin is referred to as a “low ester pectin” (“LE pectin” forshort) or a “low methoxyl pectin”. If 50% of the carboxyl groups areesterified then the resultant pectin is referred to as a “medium esterpectin” (“ME pectin” for short) or a “medium methoxyl pectin”. If thepectin does not contain any—or only a few—esterified groups it isusually referred to as pectic acid.

[0005] LE pectins have for a long time been used in yoghurt fruit as astabilising agent to ensure a certain yield stress and consequentlyuniform distribution of fruit without giving a too high viscosity.However, LE pectins tend to form a gel and any gelation should beavoided.

[0006] Gelation is detrimental to the appearance of many food productsand may also result in undesirable organoleptic properties. Gelation ofa product may also prohibit the pumping of that product. Pumping is awidely used method for manipulating products during manufacture andapplication, and consequently pumpability is a demand in manyapplications, e.g. yoghurt fruit application.

[0007] The prior art has attempted to overcome the above problems. Theprior art has provided “pregelled” systems which although they mayovercome some of the above problems, produce a product which is grainywith a dull appearance. Furthermore, such pregelled products has astrong tendency to syneresis.

[0008] The present invention aims to overcome the problems of the priorart.

[0009] According to a first aspect of the present invention there isprovided use of a pectin composition to prepare an aqueous compositionhaving high yield stress characteristics without substantial gelation,wherein the pectin composition comprises at least a population of pectinthat is calcium sensitive; wherein the pectin composition is capable ofimparting high yield stress characteristics to an aqueous compositionwithout causing substantial gelation of the aqueous composition.

[0010] The present invention is advantageous in that it may provide anaqueous composition which is smooth and shiny in appearance withoutexhibiting syneresis, in contrast to the pre-gelled systems of the priorart.

[0011] The term “pectin” includes fractions of pectin, one or morecompounds from the class of compounds known as pectins, and derivativesthereof.

[0012] The term “derivatives thereof” includes derivatised pectin anddegraded pectin (such as partially degraded pectin) and modified pectin.

[0013] The term “population of pectin that is calcium sensitive” means apopulation of pectin which has a calcium sensitivity index (CF) notequal to 1. A Protocol for determining calcium sensitivity may be foundon page 57 of WO-A-97/03574 (the contents of which are incorporatedherein by reference). For ease of reference, this Protocol is recited atthe end of the Examples section (infra) as Protocol I.

[0014] Preferably, the population of pectin has a CF of greater than1.2. More preferably, the population of pectin has a CF of greater than5. Yet more preferably, the population of pectin has a CF of greaterthan 15.

[0015] Preferably, the pectin composition has a CF of greater than 1.2.More preferably, the pectin composition has a CF of greater than 5. Yetmore preferably, the pectin composition has a CF of greater than 15.

[0016] In the present specification, by the term “having a high yieldstress” it is meant that the yield stress of the aqueous composition asmeasured in accordance with the Protocol II is at least 1.0 Pa. ProtocolII is recited at the end of the Examples section (infra).

[0017] Preferably, the yield stress of the aqueous composition isgreater than 3.0 Pa. Yet more preferably, the yield stress of theaqueous composition is greater above 5.0 Pa.

[0018] In the present specification, by the term “without substantialgelation” it is meant that the maximum viscosity of a standardisedaqueous composition measured in accordance with the Protocol III is nogreater than 500 Pa. Protocol III is recited at the end of the Examplessection (infra).

[0019] Preferably, the pectin composition is capable of imparting a highdegree of shear thinning to an aqueous composition. A high degree ofshear thinning is an important rheological characteristic in liquid andsemi-liquid systems to facilitate pumping and to secure a goodnon-sticky mouthfeel.

[0020] The degree of thixotropy of the aqueous composition may be variedfrom application to application. If stabilisation of suspended particlesis required, the aqueous composition is preferably able to build upstructure after shearing with low thixotropy. If a degree of flow aftershearing is required, a degree of thixotropy is desirable and may beprovided by the pectin composition. The pectin composition may be usedin accordance with the present invention to control the aboverheological characteristics. This control may be achieved bycontrolling, among other things, the degree of esterification (%DE), theproportion of the pectin composition which is calcium sensitive (%CSP),the calcium sensitivity of the calcium sensitive population of pectin(CS), the molecular weight of the pectin composition and/or theconcentration of calcium in the aqueous composition.

[0021] Degree of thixotropy, shear thinning and shear reversibility maybe evaluated by performing a flow curve experiment in accordance withProtocol IV. Protocol IV is recited at the end of the Examples section(infra).

[0022] Preferably, the aqueous composition has a low viscosity at ashear rate of 0.1 s⁻¹.

[0023] In the present specification, by the term “low viscosity” it ismeant that the viscosity at a shear rate of 0.1 s⁻¹, measured inaccordance with Protocol IV, is less than 100 Pa.s, preferably less than80 Pa.s.

[0024] Thus, in a second aspect the present invention provides use of apectin composition to prepare an aqueous composition having high yieldstress characteristics and a low viscosity at a shear rate of 0.1 s⁻¹,wherein the pectin composition comprises at least a population of pectinthat is calcium sensitive; wherein the pectin composition is capable ofimparting to an aqueous composition high yield stress characteristicsand a low viscosity at a shear rate of 0.1 s⁻¹.

[0025] The calcium sensitive pectin population can comprise any one ormore of a low ester pectin, a medium ester pectin or a high esterpectin. Preferably, the calcium sensitive pectin population comprises ahigh ester pectin. Preferably, the calcium sensitive pectin populationdoes not comprises a low ester pectin or a medium ester pectin.

[0026] Preferably, the degree of esterification of the calcium sensitivepectin population is from 50 to 90%. More preferably, the degree ofesterification is from 60 to 85%. More preferably, the degree ofesterification is from 60 to 80% or 65 to 85%. Yet more preferably, thedegree of esterification is from 65 to 80%.

[0027] Preferably, the degree of esterification of the total pectincomposition is from 50 to 90%. More preferably, the degree ofesterification is from 60 to 80% or 65 to 85%. Yet more preferably, thedegree of esterification is from 65 to 80%.

[0028] A Protocol for determining the degree of esterification of apectin may be found on page 58 of WO-A-97/03574 (the contents of whichare incorporated herein by reference). For ease of reference, thisProtocol is recited at the end of the Examples section (infra) asProtocol V.

[0029] The structure of pectin, in particular the degree ofesterification of pectin and the degree of block structure i.e. thedegree of distribution of ester groups and free carboxyl groups inblocks, controls many of the physical properties of the pectin. Thus,modification and/or control of the degree of esterification and degreeof block structure may be important.

[0030] The degree of esterification and/or degree of block structure maybe modified and/or controlled by any method. Examples of suitablemethods are acid hydrolysis, alkali hydrolysis, use of other chemicalde-esterification agents, or by use of enzymes. Suitable enzymes can beobtained from plants or micro-organisms such as bacteria, yeast orfungi. The enzymes disclosed in the review prepared by Pilnik andVoragen (Food Enzymology, Ed.: P. F. Fox; Elsevier; (1991); pp: 303-337)may be used.

[0031] Preferably, the degree of esterification of the pectincomposition is modified and/or controlled by use of a pectinmethylesterase (EC 3.1.1.11), otherwise referred to as a PME. PMEsde-esterify HE pectins to LE pectins or pectic acids.

[0032] The use of PMEs is advantageous because PME activity producesfree carboxyl groups and free methanol. The increase in free carboxylgroups and thus the degree of esterification can be easily monitored byautomatic titration.

[0033] For example, the degree of esterification of the calciumsensitive pectin population is modified and/or controlled in accordancewith a process described in WO 98/47391 (which claims priority fromBritish Patent Application No 9708278.8).

[0034] Preferably the pectin composition is obtainable or is obtained byfractionation of a pectin or a pectin composition. Using fractionationtechniques a pectin composition may be obtained which is enriched in oneor more specific calcium sensitive pectin populations.

[0035] Preferably the pectin composition is obtainable or is obtained byselecting peels from a citrus fruit, for instance lime and/or lemon, andextracting the pectin by a process comprising the steps of:

[0036] Extraction

[0037] Mixing the peel with water at a water:peel ratio of 21:1

[0038] Adjusting, if necessary, the pH to 1.9-2.3 using nitric acid

[0039] Heating to a temperature of 68-71° C. for 3-6 hours

[0040] Filtration

[0041] After extraction the pectin solution is filtered.

[0042] Precipitation

[0043] Reducing the temperature to 36-40° C.

[0044] Adjusting the pH to 2.6-2.9

[0045] Adding isopropyl alcohol until precipitation occurs. Typically anisopropyl alcohol concentration of 49-58 w/w % is required.

[0046] Post Treatments

[0047] After precipitation the pectin may be dried and/or milled.

[0048] Preferably, the use of the present invention provides an aqueouscomposition.

[0049] Thus, in a third aspect of the present invention there isprovided an aqueous composition prepared in accordance with the use ofthe present invention.

[0050] The aqueous composition of the present invention may comprise oneor more other components, such as one or more suitable food ingredients.Typical food ingredients include any one or more of a salt, a protein,an acid—such as citric acid—or a sugar—such as sucrose, glucose orinvert sugar—or fruit—or enzymes.

[0051] The present invention can be used in the preparation ofpharmaceutical products, foodstuffs and non-food products.

[0052] Typical pharmaceutical products include clinical nutritiveproducts (enteral products and other liquid products).

[0053] Typical non-food products include de-icing agents and paints.

[0054] The term “foodstuff” can include food for human and/or animalconsumption.

[0055] Typical foodstuffs include jams, fruit preparations, fruitfillings, ripples, fruit sauces, stewed fruit, dairy products (such asmilk products and ice cream), fine foods (such as salad dressings,ketchup, vinaigrette dressings and soups), meat products, poultryproducts, fish products and bakery products. The foodstuff may be abeverage. The beverage may be a drinking yoghurt, a fruit juice, abeverage concentrate or a fruit based beverage.

[0056] The present invention may be used in the preparation of astarting reagent or an intermediate in the preparation of a foodstuff.

[0057] Alternatively, present invention may be used in the preparationof a foodstuff itself.

[0058] Preferably, the pectin composition comprises no greater than 5.0wt % of aqueous composition based on the total weight of the aqueouscomposition. More preferably, the pectin composition comprises nogreater than 0.1-1.5 wt % of aqueous composition based on the totalweight of the aqueous composition.

[0059] Preferably, the pectin composition and/or the aqueous compositionfurther comprises one or more metal ions. Preferably, the one or moremetal ions comprise metal ions selected from ions of elements of GroupII of the Periodic Table. Yet more preferably, the one or more metalions comprise at least Ca²⁺ ions.

[0060] In a further preferred embodiment, the pectin composition and/oraqueous composition comprises 25-300 mg of metal ions per gram ofpectin. In yet a further preferred embodiment, the pectin compositionand/or aqueous composition comprises 50-150 mg of metal ions per gram ofpectin.

[0061] In a further preferred embodiment, the pectin composition and/oraqueous composition comprises 25-300 mg of Ca²⁺ ions per gram of pectin.In yet a further preferred embodiment, the pectin composition and/oraqueous composition comprises 50-150 mg of Ca²⁺ ions per gram of pectin.

[0062] In the above embodiment the metal ions may be introduced in tothe pectin composition by adding the metal ions to the pectincomposition during production thereof or it can be added to the drypectin composition afterwards. In one alternative, the metal ions may beintroduced in to the pectin composition by adding the metal ions to thepectin composition in the presence of water.

[0063] The metal ions may be introduced in to the aqueous composition byadding the metal ions directly thereto before or after the introductionof the pectin composition in to the aqueous composition.

[0064] The metal ions, preferably calcium, may be added as a metal ionsalt. For example the metal ion may be added in the citrate form of themetal, for example, calcium citrate.

[0065] An example of the combination of metal ions and pectincomposition in accordance with the present invention to provide anaqueous composition in accordance is given below:

[0066] 1) A pectin with a pH value of 5 is mixed with calcium citrate

[0067] 2) The mixture is dissolved in water. Under the pH conditionsi.e. a pH of 5, only the pectin will dissolve.

[0068] 3) The pH is lowered to a level below 4. On lowering pH thecalcium citrate will dissolve, releasing the calcium. Once the calciumis released it will become available and an aqueous compositionexhibiting high yield stress characteristics without substantialgelation is obtained.

[0069] It is essential that the pectin composition for use in thepresent invention comprises a population of pectin that is calciumsensitive. However, the pectin composition for use in the presentinvention may further comprise at least one calcium insensitive pectin.

[0070] Preferably, the population of pectin that is calcium sensitivecomprises at least 40 wt % of the pectin composition. More preferably,the population of pectin that is calcium sensitive comprises at least 50wt % of the pectin composition. More preferably, the population ofpectin that is calcium sensitive comprises at least 60 wt % of thepectin composition. More preferably, the population of pectin that iscalcium sensitive comprises at least 70 wt % of the pectin composition.Yet more preferably, the population of pectin that is calcium sensitivecomprises at least 80 wt % of the pectin composition.

[0071] The proportion of the pectin composition that is calciumsensitive may be determined in accordance with the method of ProtocolVI. Protocol VI is recited at the end of the Examples section (infra).

[0072] Preferably, the pectin composition has a reduced viscosity of atleast 0.25 L/g. More preferably, the pectin composition has a reducedviscosity of at least 0.375 L/g. Yet more preferably, the pectincomposition has a reduced viscosity of at least 0.50 L/g. Reducedviscosity may be measured in accordance with Protocol VII. Protocol VIIis recited at the end of the Examples section (infra).

[0073] In the present specification we have described that the presentinvention relates to the use of a pectin composition. However, thepresent invention also encompasses the use of any polysaccharide toprovide the advantageous properties of the present invention. Thus, in abroad aspect, the present invention provides the use of a polysaccharidecomposition to prepare an aqueous composition having high yield stresscharacteristics without substantial gelation; wherein the polysaccharidecomposition is capable of imparting high yield stress characteristics toan aqueous composition without causing substantial gelation of theaqueous composition.

[0074] Alternatively, in a broad aspect the present invention providesthe use of a composition comprising a pectin isostere to prepare anaqueous composition having high yield stress characteristics withoutsubstantial gelation, wherein the pectin isostere composition is capableof imparting high yield stress characteristics to an aqueous compositionwithout causing substantial gelation of the aqueous composition.

[0075] In a further broad aspect the present invention provides a pectincomposition, wherein the pectin composition comprises at least apopulation of pectin that is calcium sensitive; wherein the pectincomposition is capable of imparting high yield stress characteristics toan aqueous environment without causing substantial gelation of theaqueous environment. In this broad aspect the present invention furtherprovides a process for preparing an aqueous composition, preferably afoodstuff, comprising the step of combining an aqueous medium with apectin composition, wherein the pectin composition comprises at least apopulation of pectin that is calcium sensitive; wherein the pectincomposition is capable of imparting high yield stress characteristics toan aqueous environment without causing substantial gelation of theaqueous environment.

[0076] The invention will now be described, by way of example only, withreference to the accompanying drawings in which:

[0077]FIG. 1 is a graph of the analysis of a composition.

[0078]FIG. 2 is a graph of the analysis of a composition.

[0079]FIG. 3 is a graph of the analysis of a composition.

[0080]FIG. 4 is a graph of the analysis of a composition.

[0081]FIG. 5 is a graph of the analysis of a composition.

[0082]FIG. 6 is a graph of the analysis of a composition.

[0083]FIG. 7 is a graph of the analysis of a composition.

[0084]FIG. 1 shows a yield stress measurement of a pectin compositionfor use in accordance with the present invention. The procedure formeasuring yield stress is described in Protocol II. The yield stress isdetermined as the force needed (Pa) to break down the structure (pointof maximum viscosity). It is seen that the yield stress is rather high,and the viscosity is low (500 Pa s) at structure breakage. It isfurthermore seen that the viscosity curve is bell shaped in naturemeaning that the breakdown of structure only gradually takes place atstress levels higher than the yield stress. This is a characteristicproperty of pectin compositions which may be used in accordance with thepresent invention. The property means in practice that the pectincomposition, even at higher stress levels than the yield stress, retainsa substantial part of its structure and thereby stabilising ability. Inquantitative terms this is seen as a rather high viscosity and low shearrate measured at stresses somewhat above the yield stress.

[0085] In a preferred aspect the pectin composition of the presentinvention has a shear rate of no greater than 500 ml/s at a stress value2 Pa higher than the yield stress when measured in accordance withProtocol II. This behaviour is completely different from a soft gelledand brittle texture typically obtained by gelling hydrocolloids, wherethe viscosity curve after passing the yield stress point shows fastreduction of viscosity and the shear rate is increased strongly,illustrating complete loss of stabilising ability. Visually suchproducts are evaluated as brittle gels. FIG. 1 may be compared with FIG.2 which shows a yield stress measurement of an aqueous composition of alow ester amidated pectin, where a pregelled texture is obtained toavoid gelling. Such an aqueous composition of a low ester amidatedpectin composition would typically be used in food applications. Eventhough a bell shaped yield stress curve is obtained indicatingstabilising ability even somewhat above the yield stress, the aqueouscomposition of the low ester amidated pectin composition isdisadvantageous due to the very high viscosity at the yield stress.Moreover the aqueous composition of low ester amidated pectincomposition is disadvantageous, because it is dull and grainy.

[0086] When FIG. 1 is compared to FIG. 3 it can be seen that the yieldstress level, bell shaped viscosity curve and viscosity at structurebreakage of the pectin composition for use in the present invention arecomparable with that obtained when using a 0.7% xanthan composition.FIG. 1 may be compared in a similar manner to FIG. 7 illustrating theyield stress measurement of a 0.8%-xanthan composition.

[0087] Thus the pectin composition for use in the present inventionprovides an aqueous composition having high yield stress and still a lowviscosity, and furthermore the appearance of the aqueous composition issmooth and shiny, in contrast to the product obtained using low esteramidated pectin.

[0088]FIG. 4 is a graph of the viscosity at varying shear rates (“flowcurves”) of a yoghurt fruit recipe prepared in accordance with thepresent invention. The procedure for measuring flow curves is describedin protocol IV. For comparison, flow curves are also produced on thesame yoghurt fruit recipe, where the pectin composition has beensubstituted with 0.55% low ester amidated pectin or 0.7% xanthan. It canbe seen, that the viscosity at low shear rates (e.g. 0.1 s⁻¹) for theaqueous composition comprising pectin composition used in the presentinvention is lower than for the aqueous composition comprising low esteramidated pectin and more comparable with xanthan.

[0089] Two aqueous compositions, one containing a pectin compositionconsisting of calcium sensitive pectin population and the othercontaining a pectin composition consisting of a non-calcium sensitivepectin population were produced to document the importance of thepresence of a calcium sensitive pectin population. A high ester pectinraw material was fractionated into two pectin compositions. One of thepectin compositions (referred to as CSP composition) contained almostpure calcium sensitive pectin (CSP), determined in accordance with themethod of Protocol VI. The other pectin composition (referred to as NCSPcomposition) contained 0% CSP (100% non calcium sensitive pectin(NCSP)). The CSP composition and NCSP composition were tested for yieldstress properties in accordance with Protocol II. A fixed dosage of0.75% CSP and 0.75% NCSP were used, respectively.

[0090]FIGS. 5 and 6 shows the yield stress values obtained. Thesefigures demonstrate that the presence of a calcium sensitive pectinpopulation is essential in the pectin composition for use in the presentinvention.

[0091] The preparation of a pectin in accordance with the presentinvention and its use in a composition in accordance with the presentinvention will now be described.

EXAMPLES

[0092] Preparation of Pectin

[0093] A pectin composition for use in accordance with the presentinvention may be obtained by selecting peels from a citrus fruit, forinstance lime and/or lemon, and extracting the pectin composition by aprocess comprising the steps of:

[0094] Extraction

[0095] Mixing the peel with water at a water:peel ratio of 21:1

[0096] Adjusting, if necessary, the pH to 1.9-2.3 using nitric acid

[0097] Heating to a temperature of 68-71° C. for 3-6 hours

[0098] Filtration

[0099] After extraction the pectin solution is filtered.

[0100] Precipitation

[0101] Reducing the temperature to 3640° C.

[0102] Adjusting the pH to 2.6-2.9

[0103] Adding isopropyl alcohol until precipitation occurs. Typically anisopropyl alcohol concentration of 49-58 w/w % is required.

[0104] Post Treatments

[0105] After precipitation the pectin may be dried and/or milled.

[0106] The pectin composition obtained by this process was analysed tohave the following characteristics: Degree of esterification (% DE)68.1% Loss on drying 10.6% pH 3.1 Calcium sensitivity (CF) 10.4 CSPcontent 59.1%

Example 1 Fruit Preparation with 30% Soluble Solids

[0107] A fruit preparation having a formulation shown in Table I belowwas prepared in accordance with the following procedure.

[0108] 1) Dry blend the pectin, and sugar and dissolve the blend in hotwater (80-90° C.), while agitating vigorously.

[0109] 2) Mix fruit, sugar and heat to 80-90° C.

[0110] 3) Add 1) to 2), while agitating vigorously.

[0111] 4) Heat for some time and add additional water to adjust thesolid content.

[0112] 5) Add calcium lactate (preferably as a slurry) at a minimumtemperature of 90° C. under agitation

[0113] 6) Adjust pH to 3.84.0, adjust the soluble solid content to 30%and add flavouring.

[0114] 7) Cool to 30° C. under agitation

[0115] 8) Fill at 30° C.

[0116] The fruit preparation made according to Example 1 gives a yieldstress around 3 Pa which secures very good fruit piece suspension. Atthe same time the fruit preparation has a low viscosity compared tosimilar formulations made with traditional amidated low ester pectingiving a fruit preparation with good flowability and pumpability and avery clean mouthfeel property. These properties make the fruitpreparation useful in many types of yoghurts such as stirred fruityoghurt, layered yoghurts and in twinpot systems as mentioned below.

[0117] A stirred fruit yoghurt may be prepared by mixing the fruitpreparation into yoghurt (white base), for example, in an amount of10-20 wt % based on the yoghurt.

[0118] The fruit preparation may also be used in two or multi-layeredyoghurts without the formation of a gelled layer at the interface.

[0119] The fruit preparation may also be used for twin pot systems(where the fruit preparation is in a separate section to the white baseyoghurt) giving a fruit preparation with complete fruit piece suspensionand a shiny and smooth appearance.

[0120] The fruit preparation may also be used for various dessertproducts. TABLE I Ingredients wt % Pectin composition according 1.3* tothe invention Sugar 1.8 Water 24.7 Strawberry, sliced 50.0 Sugar 20.4Calcium lactate, 5H₂O 1.5 Strawberry Flavouring 10565. NID** 0.3 Total100.0 Final pH 3.8-4.0 Final % soluble solids 30 Filling Temperature 30°C.

Example 2 Fruit Preparation with 50% Soluble Solids

[0121] A fruit preparation having a formulation shown in Table II belowwas prepared in accordance with the procedure used in Example 1. Thefruit preparation was incorporated into a yoghurt as described inExample 1.

[0122] The fruit preparation has a high yield stress and good fruitpiece suspending properties. Also this fruit preparation has aconsiderably lower viscosity compared to similar formulations made withtraditional amidated low ester pectins, resulting in good flowabilityand pumpability, and a very clean mouthfeel property.

[0123] As mentioned the fruit preparation may be used in all types ofyoghurts such as stirred fruit yoghurt, layered yoghurts and in twinpotsystems, but also in other dessert systems. TABLE II Ingredients wt %Pectin composition according 1.3* to the invention Sugar 1.4 Water 7.0Strawberry, sliced 45.0 Sugar 41.3 Water 2.2 Calcium lactate, 5H₂O 1.5Strawberry Flavouring 10565, NID** 0.30 Total 100.0 Final pH 3.8-4.0Final % soluble solids 50 Filling Temperature 30° C.

Example 3 10% Fruit Drink

[0124] A fruit drink having a formulation shown in Table III below wasprepared in accordance with the following procedure.

[0125] 1) Dry blend pectin with sugar

[0126] 2) Dissolve dry-blend in water at 80° C. by agitating vigorouslyfor 15 minutes

[0127] 3) Add fruit juice, concentrate or puree and add any remainingwater

[0128] 4) Adjust pH and add flavourings and preservatives

[0129] 5) Add calcium lactate (preferably as a slurry)

[0130] 6) Heat treat the beverage at 80-90° C. either in a continuous orin a batch system

[0131] 7) De-aerate the beverage, if necessary

[0132] 8) Cool to filling temperature and fill aseptically

[0133] The viscosity level obtained in the fruit drink is relativelylow—around 25 mPas (at a shear rate/second of 50) and is comparable to asimilar fruit drink made with a CMC and Xanthan gum stabiliser system(GRINDSTED™ JU 543 Stabiliser System available from Danisco Ingredients,Denmark) used in a 0.2% dosage.

[0134] Also the yield stress and thus the pulp stabilising effect of thepectin based sample is comparable with the CMC and Xanthan gum basedreference (0.2% dosage). TABLE III Ingredients wt % Pectin compositionaccording 0.40* to the invention Orange concentrate 2.0 Sugar 11.50Flavouring 0.3 Water 85.3 Calcium lactate, 5H₂O 0.5 Total 100.0

Example 4 Fruit Drink Concentrate

[0135] Cordial/Squash (Dilution ratio 1:9)

[0136] A dilutable fruit drink concentrate having a formulation shown inTable IV below was prepared in accordance with the following procedure.

[0137] 1) Dry blend pectin with sugar

[0138] 2) Add dry-blend to water phase

[0139] 3) Heat to 90° C. for a few minutes, while agitating

[0140] 4) Add the juice concentrate and continue the heating a fewminutes

[0141] 5) Add the calcium lactate (preferably as a slurry)

[0142] 6) Dissolve the rest of the sugar at 80° C.

[0143] 7) De-aerate under vacuum at 80° C.

[0144] a) Cool to 40° C. or below and add flavourings, preservatives andclouding agent

[0145] 9) Continue agitating until the product is homogeneous

[0146] 10) Bottle/fill

[0147] Before consumption, the concentrate has to be diluted with tapwater in a 1:9 ratio by the consumer. Thus, 1 liter of concentrate gave10 liters of a ready-to-drink beverage. The beverage is a fresh andslightly acidic fruit drink.

[0148] The texture obtained in the beverage concentrate made accordingto the present invention using the described pectin is comparable withtraditional cordial/squash based on alginate/alginic acid as thickenerand stabilising agent, used in an equivalent dosage. Thus the ability ofthe pectin based fruit drink concentrate to be diluted with water iscomparable with that of the reference sample.

[0149] The use of pectin based fruit drink concentrates will also beapplicable in sugar reduced or sugar free formulations. In suchformulations the reference will often be stabilised with xanthan gumbased stabiliser systems. TABLE IV Ingredients wt % Pectin compositionaccording to 0.3* the invention Sugar 3.0 Water 31.85 Juice concentrate65-67° Brix 15.0 Calcium lactate, 5H₂O 0.4 Sugar 47.96 Preservative (asneeded) Clouding agent (optional) 1.0 Flavourings 0.5 Total 100.0 FinalpH 3.5

[0150] If the ^(o)Brix is lower for the juice concentrate added, theformulation has to be modified to obtain the right final soluble solidcontent.

Example 5 Vinaigrette Dressing

[0151] A vinaigrette dressing having a formulation shown in Table Vbelow was prepared in accordance with the following procedure.

[0152] 1) Mix water and pectin and heat to 85° C.

[0153] 2) When pectin is dissolved cool to 30° C.

[0154] 3) Add salt, sugar and spices and herb to the solution

[0155] 4) Add oil phase to the solution

[0156] 5) Add vinegar to the solution

[0157] 6) Mix for approximately 15 minutes

[0158] 7) Add calcium lactate slurry

[0159] 8) Fill

[0160] The formulation in table V was compared with a similarformulation based on Xanthan gum in 1:1 substitution.

[0161] The dressings obtained have the same stability and appearance inan organoleptic evaluation. However the dressing made with the pectinhas a yield stress of around 1.5 Pa compared to the xanthan based samplewhich has a yield stress of more than 4 Pa.

[0162] The organoleptic evaluation also shows that the pectin basedsample has a very characteristic mouth-feel property in terms of lesssticky texture, a more clean eating property and a better flavourrelease compared to the xanthan based sample.

[0163] Viscosity measurements shows that the viscosity of the twosamples is close to each other (measured at a shear rate/sec between 50and 100). TABLE V Ingredients wt % Water 48.6 Sugar 9.00 Vinegar 10%18.00 Salt 1.00 Soya oil 22.00 Parsley flakes 0.03 Black peppergranulate 0.02 Mix of herbs 0.05 Calcium lactate, 5H₂O 0.65 Pectincomposition 0.65* according to the invention Total 100.00

Example 6 Dressing

[0164] A dressing having a formulation shown in Table VI below wasprepared in accordance with the following procedure.

[0165] 1) Blend water, sugar, potassium sorbate and salt

[0166] 2) Blend pectin, propylene glycol alginate (PGA) and starch witha little oil and add to the water phase

[0167] 3) Mix until all ingredients are fully dissolved

[0168] 4) Add egg yolk to the water phase

[0169] 5) Add calcium lactate to the water phase

[0170] 6) Emulsify the remaining of the oil into the water phase

[0171] 7) Add vinegar and mustard

[0172] 8) Fill

[0173] The dressing produced has a good body and cling, and the sametexture and stability as typical commercial formulations. TABLE VIIngredients wt % Water 50.50 Soya oil 30.00 Salt 1.50 Sugar 4.50Ultratex 4 2.00 Propylene glycol alginate (PGA) 0.20 Calcium lactate,5H₂O 0.60 Pectin composition according to 0.5* the invention Fluid eggyolk 4.00 Vinegar 12% 5.00 Mustard 1.00 Potassium sorbate 0.20 Total100.00

Example 7 Ice cream

[0174] Ice cream having the formulation shown in Table VII below wasprepared according to the following procedure:

[0175] 1) Heat all liquid ingredients to approx. 40° C.

[0176] 2) Mix pectin, emulsifier and sugar

[0177] 3) Mix the dry blend with the liquid ingredients

[0178] 4) Pasteurise at 80-85° C. for 20-40 seconds

[0179] 5) Homogenise at 80° C.

[0180] 6) Cool to ageing temperature, 4° C.

[0181] 7) Age for min. 4 hours (preferably overnight)

[0182] 8) Freeze in continuous freezer to desired overrun (100%recommended)

[0183] 9) Harden in tunnel at −40° C.

[0184] 10) Store at a temperature below −25° C.

[0185] The use of the described pectin/calcium system in the recipe willhelp reduce the ice crystal formation in the ice cream during productionand during freeze storage of the ice cream.

[0186] The ice-cream has thus a good heat-shock resistance, and a dryand creamy mouthfeel, with clean-eating properties.

[0187] The meltdown of the ice cream made according to the formulationis comparable to an ice cream made with xanthan gum (0.18%). Both ofthem have a relatively slow meltdown, and slower meltdown compared tostandard commercial ice cream.

[0188] Also the “first drop” (minutes before the ice cream starts todrip under standardised conditions) is very similar for the ice creammade with pectin and xanthan gum.

[0189] Increasing the pectin dosage to only 0.30% gives a considerablyimprovement of these described properties. TABLE VII Ingredients wt %Dairy cream, 38% milk fat 23.65 Skimmed milk 53.55 Skimmed milk powder4.90 Pectin composition according 0.25* to invention Sugar 12.00 Glucosesyrup, DE 42, 75% TS 5.35 CREMODAN ® Super 0.3 Flavouring OptionalColouring Optional Total 100.00 Fat (percent) 9.00 MSNF (percent) 10.80Total solids (percent) 36.35

Protocol I Calcium Sensitivity Index (CF)

[0190] Calcium sensitivity is measured as the viscosity of a pectindissolved in a solution with 57.6 mg calcium/g pectin divided by theviscosity of exactly the same amount of pectin in solution, but withoutadded calcium. A calcium insensitive pectin has a CF value of 1.

[0191] 4.2 g pectin sample is dissolved in 550 ml hot water withefficient stirring. The solution is cooled to about 20° C. and the pHadjusted to 1.5 with 1N HCl. The pectin solution is adjusted to 700 mlwith water and stirred. 290 g of this solution is measured individuallyinto 2 viscosity glasses. 10 ml water is added to one of the glasses(double determinations) and 10 ml of a 250 mM CaCl₂ solution is added tothe other glass under stirring.

[0192] 50 ml of an acetate buffer (0.5 M, pH about 4.6) is added to bothviscosity glasses under efficient magnetic stirring, thereby bringingthe pH of the pectin solution up over pH 4.0. The magnets are removedand the glasses left overnight at 20° C. The viscosities are measuredthe next day with a Brookfield viscometer. The calcium sensitivity indexis calculated as follows:${CF} = {\frac{\text{Viscosity of a solution with}\quad {57.6\quad {mg}\quad {Ca}^{2 +}\text{/}g\quad {pectin}}}{\text{Viscosity of a solution with}{0.0\quad {mg}\quad {Ca}^{2 +}\text{/}g\quad {pectin}}}.}$

Protocol II Yield Stress

[0193] An aqueous composition was prepared in accordance with thefollowing procedure

[0194] 1) The pectin composition was blended in hot water (80-90° C.)while agitating vigorously.

[0195] 2) Diluting concentrated strawberry juice* at a ratio of 1:6.5with water to provide strawberry juice having a solid content of 10.0%and a calcium content of 200 ppm.

[0196] 3) Mix the diluted strawberry juice and pectin composition whileagitating vigorously

[0197] 4) Heat to boiling point

[0198] 5) Add calcium lactate.5H₂O to provide a level of Ca²⁺/pectin of150 mg/g**

[0199] 6) Adjust pH to 3.8-4.0

[0200] 7) Adjust soluble solid content to 30%

[0201] 8) Cool to 30° C. under agitation to provide an aqueouscomposition

[0202] * available from Dinter Gmbh.

[0203] Specification

[0204] soluble solid content of 65%

[0205] calcium content of approximately 1300 ppm

[0206] produced by concentration of strawberry juice, obtained frompressing fresh/frozen strawberries

[0207] Brix: 64.0-66.0

[0208] Acidity: 6.0-7.8% as citric acid, pH 8.1

[0209] ** This amount of calcium lactate has been optimised for highester pectin. The amount of calcium lactate may be varied if a mediumester or low ester pectin is to be considered. This optimisation may beachieved by the performance of a series of simple experiments varyingthe amount of calcium lactate to optimise the high yieldstress/non-gelling properties of an aqueous composition containing apectin composition of the present invention.

[0210] The rheological effect of the strawberry juice concentrate isdirectly related to the amount of calcium in the juice concentrate. Theconcentrate may be analysed and replaced with a calcium solution e.g. acalcium lactate solution. The present Protocol has been repeated withsuch a solution and identical results were obtained.

[0211] The aqueous composition was stored at room temperature forminimum 48 hours and applied to a Stress Tech CS rheometer supplied byReologica Instruments AB. The pectin sample was applied as gently aspossible without stirring of the sample.

[0212] The rheometer was configured as follows Programme: Yield StressMeasurement System: CC 25 (25 mm concentric cylinders) Equilibrium time:900 s Stress: 0.1429-10.00 Pa, up Measurement time: 300.0 s in 60intervals Temperature: 25° C.

[0213] The procedure is repeated, if necessary, until the ratio ofpectin composition to water required to achieve a maximum viscosity ofapproximately 500 Pa is determined. This ratio provides a standardisedaqueous composition.

[0214] The yield stress of a standardised pectin composition is thendetermined by applying (as gently as possible without stirring of thesample) the standardised aqueous composition which has been stored atroom temperature for minimum 48 hours to a Stress Tech CS rheometersupplied by Reologica Instruments AB.

[0215] The rheometer was configured as follows Programme: Yield StressMeasurement System: CC 25 (25 mm concentric cylinders) Equilibrium time:900 s Stress: 0.1429-10.00 Pa, up Measurement time: 300.0 s in 60intervals Temperature: 25° C.

[0216] The yield stress is determined as the stress giving the maximumviscosity during stress viscometry.

Protocol III Non-gelling

[0217] An aqueous composition was prepared in accordance with thefollowing procedure

[0218] 1) The pectin composition was blended in hot water (80-90° C.)while agitating vigorously.

[0219] 2) Diluting concentrated strawberry juice* at a ratio of 1:6.5with water to provide strawberry juice having a solid content of 10.0%and a calcium content of 200 ppm.

[0220] 3) Mix the diluted strawberry juice and pectin composition whileagitating vigorously

[0221] 4) Heat to boiling point

[0222] 5) Add calcium lactate.5H₂O to provide a level of Ca²⁺/pectin of150 mg/g**

[0223] 6) Adjust pH to 3.84.0

[0224] 7) Adjust soluble solid content to 30%

[0225] 8) Cool to 30° C. under agitation to provide an aqueouscomposition

[0226] * available from Dinter Gmbh.

[0227] Specification

[0228] soluble solid content of 65%

[0229] calcium content of approximately 1300 ppm obtained from pressingfresh/frozen strawberries

[0230] Brix: 64.0-66.0

[0231] Acidity: 6.0-7.8% as citric acid, pH 8.1

[0232] This amount of calcium lactate has been optimised for high esterpectin. The amount of calcium lactate may be varied if a medium ester orlow ester pectin is to be considered. This optimisation may be achievedby ht e performance of a series of simple experiments varying the amountof calcium lactate to optimise the high yield stress/non-gellingproperties of an aqueous composition containing a pectin composition ofthe present invention.

[0233] The rheological effect of the strawberry juice concentrate isdirectly related to the amount of calcium in the juice concentrate. Theconcentrate may be analysed and replaced with a calcium solution e.g. acalcium lactate solution. The present Protocol has been repeated withsuch a solution and identical results were obtained.

[0234] The aqueous composition was stored at room temperature forminimum 48 hours and applied to a Stress Tech CS rheometer supplied byReologica Instruments AB. The pectin sample was applied as gently aspossible without stirring of the sample.

[0235] The rheometer was configured as follows Programme: Yield StressMeasurement System: CC 25 (25 mm concentric cylinders) Equilibrium time:900 s Stress: 0.1429-10.00 Pa, up Measurement time: 300.0 s in 60intervals Temperature: 25° C.

[0236] The procedure is repeated, if necessary, until the ratio ofpectin composition to water required to achieve a yield stress ofapproximately 1 Pa is determined. This ratio provides a standardisedaqueous composition.

[0237] The yield stress of a standardised pectin composition is thendetermined by applying (as gently as possible without stirring of thesample) the standardised aqueous composition which has been stored atroom temperature for minimum 48 hours to a Stress Tech CS rheometersupplied by Reologica Instruments AB.

[0238] The rheometer was configured as follows Programme: Yield StressMeasurement System: CC 25 (25 mm concentric cylinders) Equilibrium time:900 s Stress: 0.1429-10.00 Pa, up Measurement time: 300.0 s in 60intervals Temperature: 25° C.

[0239] The presence of gelation is determined by measuring the maximumviscosity during stress viscometry.

Protocol IV Flow Curve

[0240] To evaluate shear reversibility an aqueous composition asdescribed in protocol II was prepared and a flow curve was obtained inaccordance with the following.

[0241] The sample was stored at room temperature for minimum 48 hoursand applied to a Bohlin VOR rheometer. The sample was applied as gentlyas possible without stirring of the sample.

[0242] The rheometer was configured as follows Programme: ViscometryMeasurement System: CC 25 (25 mm concentric cylinders) Torque bar: 20.25gcm or 41.10 gcm Shear rate: 0.06-92 s⁻¹, up and down Equilibrium time:900 s Measurement time: 608 s in 33 intervals Temperature: 25° C.

[0243] The viscosity and shear stress as a function of shear rate isfollowed.

[0244] The viscosity profile as a function of shear rate illustrates thedegree of shear thinning of the system.

[0245] The viscosity at any given shear rate, in particular 0.1 s⁻¹ maybe readily determined.

[0246] The area between the “up” and “down” curves in the flow curvecorresponds to the degree of thixotropy.

Protocol V Degree of Esterification (%DE)

[0247] To 50 ml of a 60% isopropanol and a 5% HCl solution is added 2.5g pectin sample and stirred for 10 min. The pectin solution is filteredthrough a glass filter and washed with 15 ml 60% isopropanol/5% HClsolution 6 times followed by further washes with 60% isopropanol untilthe filtrate is free of chlorides. The filtrate is dried overnight at80° C.

[0248] 20.0 ml 0.5 N NaOH and 20.0 ml 0.5 N HCl is combined in a conicalflask and 2 drops of phenolphthalein is added. This is titrated with 0.1N NaOH until a permanent colour change is obtained. The 0.5 N HCl shouldbe slightly stronger than the 0.5N NaOH. The added volume of 0.1 N NaOHis noted as V₀.

[0249] 0.5 g of the dried pectin sample (the filtrate) is measured intoa conical flask and the sample is moistened with 96% ethanol. 100 ml ofrecently boiled and cooled distilled water is added and the resultingsolution stirred until the pectin is completely dissolved. Then 5 dropsof phenolphthalein are added and the solution titrated with 0.1 N NaOH(until a change in colour and pH is 8.5). The amount of 0.1 N NaOH usedhere is noted as V₁. 20.0 ml of 0.5 N NaOH is added and the flask shakenvigorously, and then allowed to stand for 15 min. 20.0 ml of 0.5 N HClis added and the flask is shaken until the pink colour disappears. 3drops of phenolphthalein are then added and then the resultant solutionis titrated with 0.1 N NaOH. The volume 0.1 N NaOH used is noted as V₂.

[0250] The degree of esterification (% DE: % of total carboxy groups) iscalculated as follows:${\% \quad {DE}} = \frac{V_{2} - V_{0}}{V_{1} + \left( {V_{2} - V_{0}} \right)}$

Protocol VI Method of Determining CSP Content

[0251] A pectin composition was fractionated into a calcium sensitivefraction (CSP) and a none calcium sensitive fraction (NCSP) inaccordance with the method below

[0252] Dissolve 1% sugar free pectin in water

[0253] Adjust pH to 4.5 with a solution of 10% Na₂CO₃

[0254] Make a fractionation solution of 60 mM CaCl₂/16% IPA/water

[0255] Measure 20 ml fractionation solution in a 80 ml centrifugationglass

[0256] Inject about 20 grams pectin solution into the fractionationsolution, the precise amount to be noted

[0257] Centrifuge at 5000 rpm for 20 minutes

[0258] Separate

[0259] Add 30 ml fractionation solution, diluted in a ratio of 1:1 withwater

[0260] Mix the sedimented gel and the diluted fractionation solutionwith a spatula and centrifuge at 5000 rpm for another 5 minutes

[0261] Repeat this procedure twice

[0262] Dissolve the gel with a few drops of 3 N HCl and stir with aspatula

[0263] Add 60 ml 60% IPA/3% HCl/37% H₂O to the dissolved gel. Mix andcentrifuge at 5000 rpm for 5 minutes

[0264] Wash out chloride from the material with 60 ml 60% IPA fourtimes. Each wash is mixed, centrifuged and separated

[0265] The CSP fraction is transferred to a low weight plastic petridish (which has been weighed on beforehand)

[0266] Dry at 40° C. over night

Protocol VII Reduced Viscosity

[0267] A quantity of pectin corresponding to 90 mg pectin dry matter isweighted into a 150 ml Erlenmeyer flask together with 100 g buffersolution which is prepared by dissolving 1 g sodium hexametaphosphate indistilled water and adjusting the pH value to 4.5 with a few drops of 4NHCL. After a few hours of stirring the pectin is dissolved. If it is notclear the solution is filtered through a porosity 2-filter crucible.Dropping periods of the resulting pectin solution and the buffersolution, respectively are measured at 20° C. in a “falling ballviscometer” (Hoeppler viscometer)

[0268] The specific viscosity is:

η_(sp)=(Dropping period for pectin solution/dropping period for buffersolution)−1

1. Use of a pectin composition to prepare an aqueous composition havinghigh yield stress characteristics without substantial gelation, whereinthe pectin composition comprises at least a population of pectin that iscalcium sensitive; wherein the pectin composition is capable ofimparting high yield stress characteristics to an aqueous compositionwithout causing substantial gelation of the aqueous composition.
 2. Useaccording to claim 1 wherein the pectin composition comprises no greaterthan 5.0 wt % of the aqueous composition based on the total weight ofthe aqueous composition.
 3. Use according to claim 2 wherein the pectincomposition comprises no greater than 0.1-1.5 wt % of the aqueouscomposition based on the total weight of the aqueous composition.
 4. Useaccording to any one of claim 1 , 2 or 3 wherein the aqueous compositioncomprises Ca²⁺ ions.
 5. Use according to claim 4 wherein the aqueouscomposition comprises 25-300 mg of Ca²⁺ ions per gram of pectincomposition.
 6. Use according to claim 4 wherein the aqueous compositioncomprises 50-150 mg of Ca²⁺ ions per gram of pectin composition.
 7. Useaccording to any one of the preceding claims wherein the aqueouscomposition has a low viscosity at a shear rate of 0.1 s⁻¹.
 8. Anaqueous composition prepared in accordance with any one of the precedingclaims.
 9. Use as substantially described herein with reference to anyone of the Examples.
 10. An aqueous composition as substantiallydescribed herein with reference to any one of the Examples.